反应详情

A mixture of PyBOP (0.08 mmol in 200 mL of DMF), {[3′-(1-piperazinylmethyl)-3-biphenylyl]methyl}amine (44 mmol in 200 mL of DMF) and DIPEA (30 mL) were added to [4-(dimethylamino)phenyl]acetic acid (0.07 mmol). The resulting mixture was stirred for 16 hours at room temperature, then the solvent was removed under vacuum. The residue was dissolved in methanol and purified by loading onto a SPE cartridge (SCX, 500 mg), washing with MeOH, and eluting with a 2 M solution of NH3 in MeOH. The NH3 fraction was collected and evaporated under vacuum to give a gum which was dissolved in 1:1 CHCl3/TFA (0.5 mL). After stirring for 2 hours, the solvent was removed under vacuum and the residue was dissolved in MeOH. The free base of the compound was obtained by loading the solution onto a SPE cartridge (SCX, 500 mg), washing with MeOH, and eluting with 2M NH3/MeOH. The ammonia fraction was collected and the solvent was removed under vacuum to give the title compound (14.6 mg). LC/MS: m/z, 443 (M+H), 2.21 min.

1. customthe solvent was removed under vacuum
2. dissolutionThe residue was dissolved in methanol
3. custompurified
4. washwashing with MeOH
5. washeluting with a 2 M solution of NH3 in MeOH
6. customThe NH3 fraction was collected
7. customevaporated under vacuum
8. customto give a gum which
9. stirringAfter stirring for 2 hours
10. customthe solvent was removed under vacuum
11. dissolutionthe residue was dissolved in MeOH
12. customThe free base of the compound was obtained
13. washwashing with MeOH
14. washeluting with 2M NH3/MeOH
15. customThe ammonia fraction was collected
16. customthe solvent was removed under vacuum